[气相色谱-质谱法测定蘑菇中的福美双、丙森锌和代森联]

[Determination of thiram, propineb and metiram in mushroom by gas chromatography-mass spectrometry].

作者信息

Zhang Jing, Tan Ying, Feng Liang, Ni Zhunan, Wang Junlin, Cai Zengxuan

机构信息

Zhejiang Center for Disease Control and Prevention, Hangzhou 310051, China.

出版信息

Wei Sheng Yan Jiu. 2020 Mar;49(2):267-271. doi: 10.19813/j.cnki.weishengyanjiu.2020.02.017.

DOI:10.19813/j.cnki.weishengyanjiu.2020.02.017

PMID:32290944

Abstract

OBJECTIVE

To establish a method for determination of thiram, propineb and metiram in mushroom samples by gas chromatography-mass spectrometry(GC-MS).

METHODS

Insoluble heavy metal salts were converted into water-soluble sodium salts by alkaline buffer with strong chelating agents. Dithiocarbamates can be converted into different methyl ester compounds with ion pair methylation. The GC separation was performed on a DB-5 MS capillary column(30 m×0. 25 mm, 0. 25 μm). The pesticides were detected by GC-MS with selective ion monitoring(SIM) and quantified by external standard of working curve method. Methodsological verification was carried out based on optimized sample pretreatment and GC-MS condition.

RESULTS

The concentrations of dithiocarbamates exhibited a good linear relationship with GC-MS within a certain range. The limits of detection of thiram, propineb and metiram were 0. 01, 0. 05 and 0. 05 mg/kg, respectively. Furthermore, the average recoveries were from 76. 98% to 93. 52%, and the maximum relative standard deviation was 11. 54%(n=6).

CONCLUSION

This method is simple, sensitive, accurate and reliable. All the indices meet the requirements of pesticide residue detection.

摘要

目的

建立气相色谱 - 质谱联用（GC-MS）法测定蘑菇样品中福美双、丙森锌和代森联的方法。

方法

用含强螯合剂的碱性缓冲液将不溶性重金属盐转化为水溶性钠盐。二硫代氨基甲酸盐可通过离子对甲基化转化为不同的甲酯化合物。采用DB-5 MS毛细管柱（30 m×0.25 mm，0.25 μm）进行GC分离。通过GC-MS采用选择离子监测（SIM）模式检测农药，并采用工作曲线外标法进行定量。基于优化后的样品前处理和GC-MS条件进行方法学验证。